CN103614582A - Method for producing manganese nitride product - Google Patents
Method for producing manganese nitride product Download PDFInfo
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Abstract
The invention discloses a method for producing a manganese nitride product. A material temperature rise stage or/and a cooling process at the end of the highest-temperature reaction stage are divided into two stages. More specifically, any one or two points exit as follows: 1) the material temperature rise stage is divided into two stages: an initial temperature rise stage and a continuous heating stage; 2) nitrogen is fed when the system reaches 650-700 DEG C in the initial temperature rise stage; 3) the cooling process at the end of the highest-temperature reaction stage is divided into two stages, when the temperature is higher than 650 DEG C, the cooling speed is 1-3 DEG C/min and the nitrogen pressure is kept at 0.4-1.0 MPa, and after the temperature is lower than 650 DEG C, the cooling speed is 3-10 DEG C/min, and the nitrogen valve is closed. The nitrogen content of the manganese nitride product produced by using the process is 8-12%, and the nitrogen content fluctuation of a single batch of products is smaller than +/- 0.5%.
Description
Technical field
The present invention relates to a kind of smelting technology of nitrogenized manganese alloy, specifically belong to the technical field of iron alloy metallurgical engineering.
Background technology
Well-known: " without manganese Cheng Gang not ".Iron And Steel Industry accounts for 90% ~ 95% of manganese output to the demand of manganese.Manganese is reductor, sweetening agent and alloy element important in steelmaking process.Manganese energy reinforced ferrite and refine pearlite, thus intensity and the hardening capacity of steel can be improved, thereby can be used as the alloying element of steel.Manganese mainly adds molten steel in the mode of iron alloy in smelting process.In the last few years, the effect of nitrogen was also more and more subject to people's attention.Such as: 1, in polycomponent stainless steel, the effect that nitrogen can part replacement nickel forms stable austenite structure, improves the macrostructure of steel, and forms nitride with alloying element, thereby improves intensity, hardness, corrosion-resistant and the welding property of steel; 2, in the high nitrogen steel of novel material, along with the increase of nitrogen content, the yield strength of steel increases, and work hardening also significantly increases, and the mechanics of high nitrogen steel and corrosive nature are much better than without nitrogen steel.Because nitrogen directly adds molten steel very difficult, and nitrogenized manganese product can add manganese element and nitrogen element simultaneously in molten steel, so nitrogenized manganese product is more and more subject to the attention of the ferroalloy industry.
The production technique of current domestic nitrogenized manganese mainly adopts the mode of vacuum electric heating stove batch machining.The preparation method of the nitrogenize Mn series alloy that such as CN102080169A, CN101082088A, CN1799991A, CN1803585A etc. announced, its common feature is: adopt vacuum nitriding furnace, without inner bag frame, pack in batches, the temperature in control process, pressure and other parameters obtain nitrogenized manganese product.A common ground of these methods is: charging in enormous quantities, for a long time reaction and cooling.The shortcoming of this method is: 1, because the nitrogenize whole process using electrically heated of manganese metal, so energy consumption is very high; 2, owing to having thermal insulation layer and refractory materials in vacuum oven, cause furnace charge rate low, equipment is huge, and nitrogen pressure improves difficulty; When 3, cooling, owing to cannot opening fire door (preventing manganese high temperature oxidation), so cooling time is long, efficiency is low; 4, body of heater must could be feeded through overcooling at every turn again, causes body of heater intensification energy wastage.
According to Mn-N phasor, the solubleness in is mutually along with the reduction of temperature raises at high temperature ζ for nitrogen, otherwise temperature raises, nitrogen content reduces.According to Mn-N reaction power theory, the rising of temperature can be accelerated the speed of response of Mn-N system in addition.Once therefore above-mentioned some patent thinks that arriving maximum temperature is exactly the sign that reaction finishes, what even have has just cut off source nitrogen at 800 ℃, thereby causes owing to there is no sufficient time absorbed nitrogen in process of cooling, so nitrogen content is not high.The nitrogen content that general these techniques can reach is all lower than 7%.Owing to there is no the sufficient reaction times, cause the manganese metal nitrogen content of different positions in reaction vessel also different equally, general fluctuation range is 4% ~ 7%.
Summary of the invention
The object of the invention is for the deficiency in background technology, the object of the invention is to provide the novel method of the nitrogenized manganese product that a kind of production efficiency is high, nitrogen content is high, reliability of technology is high, energy consumption is low.
The problem existing for reaching above-mentioned prior art, the production method of a kind of nitrogenized manganese product of the present invention, is characterized in that, the described material temperature rise period is or/and the temperature-fall period of highest temperature step of reaction after finishing is divided into two stages.
Further, the production method of described nitrogenized manganese product, is characterized in that, has the combination of following any point or multiple spot:
1) material heats up and is divided into two stages, initial temperature rise period and continuous heating stage: the mode that the initial temperature rise period adopts is: the material using manganese metal raw material as question response packs in retort, and confined reaction tank, retort is packed into normal pressure gas heating furnace, control 1000 ± 10 ℃ of furnace temperature; When temperature of charge reaches 800 ℃ ~ 900 ℃, start the continuous heating stage, the mode in continuous heating stage is: retort is taken out and packed pressure electrothermal oven into and sealing is fixed from gas furnace, continuous heating to 950 ℃ ~ 1000 ℃;
2) the initial temperature rise period, when material reaches 650 ℃ ~ 700 ℃, just passes into nitrogen;
3) temperature-fall period of highest temperature step of reaction after finishing is divided into two stages, the rate of temperature fall of temperature during higher than 650 ℃ is 1 ~ 3 ℃/min, and nitrogen pressure remains on 0.4MPa ~ 1.0MPa, temperature be down to 650 ℃ following after, rate of temperature fall is 3 ℃/min ~ 10 ℃/min, and closes nitrogen valve.
By high-power intensification, adopt cheap Sweet natural gas, and small power insulation adopts electricity, and material passes into nitrogen once reaching nitrogenize initial temperature, utilize the hot help system of nitrogenizing reaction to heat up, saved energy; Simultaneously this two-part heats up and also makes to produce and be achieved continuously in batches.
The production method of described a kind of nitrogenized manganese product, specifically comprises the steps:
1) manganese metal raw material is packed in retort, and confined reaction tank, retort is evacuated to absolute pressure 50Pa ~ 100Pa simultaneously.The feature of this step is: manganese metal raw material can directly pack in confined reaction tank, does not need extra pallet and framework;
2) mode by the initial temperature rise period makes the temperature of charge in retort rise to 650 ℃ ~ 700 ℃, passes into nitrogen, and to keep retort internal pressure scope be 0.01MPa ~ 0.03MPa.When manganese metal raw material reaches nitrogenizing reaction starting temperature, (650 ℃ ~ 700 ℃) just pass into nitrogen, make full use of nitrogenizing reaction heat and improve system temperature, and save energy and shorten heat-up time, enhances productivity.Select low pressure can avoid damaging confined reaction tank, extend its work-ing life;
3) when the temperature of charge in retort reaches 800 ℃ ~ 900 ℃, adopt the mode continuous heating to 950 ℃ in continuous heating stage ~ 1000 ℃, allow the pressure of pressure electrothermal oven internal pressure and retort identical simultaneously, and be controlled at 0.4MPa ~ 1.0MPa.Higher temperature of charge and higher nitrogen pressure condition promote that nitrogenizing reaction carries out fast, thereby enhance productivity.
4) in retort, temperature of charge reaches 950 ℃ ~ 1000 ℃, when nitrogen pressure is 0.4MPa ~ 1.0MPa, and the nitrogen flow that passes into retort be less than peak flow 1% time, control temperature according to the rate of temperature fall cooling of 1 ~ 3 ℃/min, nitrogen pressure still remains on the scope of 0.4MPa ~ 1.0MPa.Under stable high temperature pressure state, when flow drops to 1% of peak flow, illustrate that nitrogenizing reaction has been tending towards stopping substantially.Using this flux values as judgment basis, trigger stove heating schedule and start according to the cooling of 1 ~ 3 ℃/min rate of temperature fall, through the approximately cooling of 2 ~ 4hr, nitrogen content still has 1 ~ 2% weightening finish.This step allows novel process of the present invention improve 1 ~ 2% than the nitrogen content of traditional technology.
5) when the temperature of the material in retort drops to 650 ℃, close nitrogen valve, the pressure of relief pressure electrothermal oven is to normal pressure, and retort is taken out, and packing cooling shaft into, to carry out water smoke air-cooled, controls rate of temperature fall between 3 ℃/min ~ 10 ℃/min.Close nitrogen for 650 ℃ that at nitrogenizing reaction, substantially stop, and make retort separated with pressure electrothermal oven, make retort in this temperature, can be good at carrying out cooling fast, and be unlikely to damage container, affect the life-span.And cooling with water smoke wind in cooling shaft, the furnace cooling of comparing traditional technology has improved cooling rate greatly, thereby has significantly improved production efficiency.
6), when the temperature of the material in retort is reduced to below 200 ℃, retort is opened in pressure release.Whole process keeps malleation to avoid oxygen to enter retort, has improved the stability of technique.
7) pour out material and obtain nitrogenized manganese product, finishing warehouse-in.
Step 2) heating mode used in, for retort is packed into normal pressure gas heating furnace, is controlled 1000 ± 10 ℃ of furnace temperature, and advantage is: 1, adopt heated by natural gas, than electrically heated, reduced production cost; 2, this gas furnace adopts heat accumulating type or pre-heated mode to carry out energy recovery, has further reduced energy consumption, has improved energy utilization rate; 3, because retort does not need furnace cooling, this gas furnace can keep the condition of high temperature always, and laser heating subsequent reactions tank, so stove does not need, for self heating and cooling consumed energy and time, greatly to have improved economy and the efficiency of technique;
When the temperature in step 3) reaches 800 ℃ ~ 900 ℃, the mode of continuous heating is: retort is taken out and packed pressure electrothermal oven into and seal fixing from gas furnace, continuous heating to 950 ℃ ~ 1000 ℃, advantage is: when system temperature reaches more than 800 ℃, the obvious speedup of nitrogenizing reaction, system nitrogenizing reaction liberated heat obviously increases, required heating power obviously declines, now only need lower insulation power, now retort proceeds to low power electrothermal oven from powerful gas furnace, corresponding process is exactly that high-power intensification proceeds to small power insulation, this process device utilization is reasonable, energy conservation.
Further, described in step 1), manganese metal raw material is any one or the multiple mixing in electrolytic metal Mn sheet, manganese powder, manganese metal ball or metal manganese block.
Further, described manganese metal material, is characterized in that: manganese metal ball is to form by adding water glass pressure forming after the fragmentation of manganese metal sheet.
Further, the nitrogenized manganese product that described method is produced, is characterized in that: the mass content scope of nitrogen is 8% ~ 12%, and the single batch of product nitrogen content fluctuation be less than ± 0.5%.
Nitrogenized manganese product processes of the present invention, than prior art, has following advantage:
1) in nitrogenize, arrive after top temperature, begin to cool down in process, adopt controlled cooling technology controlling and process rate of cooling and nitrogen pressure, thereby guarantee have time enough to absorb enough nitrogen in suitable temperature, thus the leeway that the nitrogen content in nitrogenized manganese is improved.Compare traditional cooling not controlled technique, improved the content of finished product nitrogen, dwindled the fluctuation range of nitrogen content, thereby significantly improved benefit and quality.
2) adopt Sweet natural gas as fuel, sealed reaction tank is as carrier, realized under normal pressure starvation preheating manganese metal raw material to 800 ℃ of nitrogenizing reaction temperature.Compare traditional whole process electrically heated, greatly reduce energy cost.
3) technological design compact and reasonable, efficiency and remarkable benefit improve.Two stages of material preheating and high temperature pressure nitrogenize have realized separated by gas furnace with pressure electrothermal oven cleverly.High-power normal pressure preheating and the insulation of small power high temperature pressure, the division of labor is clear and definite, and technique is compact, can realize the production of continuous and compact in batches, and hourly output is high, introduces heated by natural gas simultaneously and has reduced nitrogenize cost.Compare traditional technology, in process of production, hot equipment does not need cooling, so conserve energy.
4) cooling quick, efficiency increases.Owing to adopting confined reaction tank, so retort can be put into cooling shaft, take coolingly fast, greatly shortened cooling time, improved production efficiency.
5) what the present invention adopted is not add additivated method, thus more easily realize, and there is no the shortcoming of the increase of cost and the pollution of material.
Embodiment
Embodiment 1
One ton of manganese ball raw material packs in retort and sealing, is evacuated to absolute pressure 100Pa, and puts into gas heating furnace, and Control for Kiln Temperature is at 1000 ± 10 ℃.When through 1 hour, ，Dang manganese ball center temperature reached 650 ℃, vacuum breaker passes into nitrogen, and to control nitrogen pressure be 0.01MPa.When manganese bulb temperature reaches 800 ℃, retort is packed into pressure electrothermal oven, airtight connection is also fixing, control stove power Shi Meng ball center temperature within 950 ℃ ~ 960 ℃ scopes, synchronization control pressure electrothermal oven and retort internal pressure reach 0.4MPa, after 1.0 hours, nitrogen flow is reduced to 0.8% of peak flow, starts cooling.Controlling rate of temperature fall is 3.0 ℃/min, and pressure still keeps 0.4MPa, and after 1.8 hours, temperature is down to 650 ℃.Relief pressure electrothermal oven pressure is to normal pressure, and removes retort and connect, and handling retort is to water smoke cooling shaft, and high speed is cooling.Through 0.8 hour cooling, material core temperature reaches below 200 degree, retort is opened in pressure release, pours out material, broken vanning.After testing, product averaged nitrogen content is 8.1%, and retort center nitrogen content is 8.3%, and retort wall place nitrogen content is 8.0%, nitrogen content fluctuation is less than ± and 0.5%.
Embodiment 2
One ton of electrolytic manganese tablet raw material packs in retort and sealing, is evacuated to absolute pressure 50Pa, and puts into gas heating furnace, and Control for Kiln Temperature is at 1000 ± 10 ℃.Through 1.2 hours, when manganese sheet core temperature reaches 700 ℃, vacuum breaker passed into nitrogen, and to control nitrogen pressure be 0.02MPa.When manganese sheet temperature reaches 900 ℃, retort is packed into pressure electrothermal oven, airtight connection is also fixing, control stove power Shi Meng ball center temperature within 990 ℃ ~ 1000 ℃ scopes, synchronization control pressure electrothermal oven and retort internal pressure reach 0.7MPa, after 2.0 hours, nitrogen flow is reduced to 1% of peak flow, starts cooling.Controlling rate of temperature fall is 2.0 ℃/min, and pressure still keeps 0.7MPa, and after 2.8 hours, temperature is down to 650 ℃.Relief pressure electrothermal oven pressure is to normal pressure, and removes retort and connect, and handling retort is to water smoke cooling shaft, and high speed is cooling.Through 1.5 hours cooling, material core temperature reaches below 200 degree, retort is opened in pressure release, pours out material, broken vanning.After testing, Nitrogen in Products content is 10.2%.Retort center nitrogen content is 10.4%, and retort wall place nitrogen content is 9.8%, nitrogen content fluctuation is less than ± and 0.5%.
Embodiment 3
One ton of electrolytic manganese powder raw material packs in retort and sealing, is evacuated to absolute pressure 75Pa, and puts into gas heating furnace, and Control for Kiln Temperature is at 1000 ± 10 ℃.Through 1.3 hours, when manganese powder core temperature reaches 675 ℃, vacuum breaker passed into nitrogen, and to control nitrogen pressure be 0.03MPa.When manganese sheet temperature reaches 850 ℃, retort is packed into pressure electrothermal oven, airtight connection is also fixing, control stove power Shi Meng ball center temperature within 970 ℃ ~ 980 ℃ scopes, synchronization control pressure electrothermal oven and retort internal pressure reach 1.0MPa, after 3.0 hours, nitrogen flow is reduced to 0.9% of peak flow, starts cooling.Controlling rate of temperature fall is 1.5 ℃/min, and pressure still keeps 1.0MPa, and after 3.5 hours, temperature is down to 650 ℃.Relief pressure electrothermal oven pressure is to normal pressure, and removes retort and connect, and handling retort is to water smoke cooling shaft, and high speed is cooling.Through 2.0 hours cooling, material core temperature reaches below 200 degree, retort is opened in pressure release, pours out material, broken vanning.After testing, Nitrogen in Products content is 11.5%.Retort center nitrogen content is 11.8%, and retort wall place nitrogen content is 11.2%, nitrogen content fluctuation is less than ± and 0.5%.
Claims (7)
1. a production method for nitrogenized manganese product, is characterized in that, the described material temperature rise period is or/and the temperature-fall period of highest temperature step of reaction after finishing is divided into two stages.
2. the production method of nitrogenized manganese product according to claim 1, is characterized in that, has the combination of following any point or multiple spot:
1) material heats up and is divided into two stages, initial temperature rise period and continuous heating stage; Wherein, the mode that the initial temperature rise period adopts is: the material using manganese metal raw material as question response packs in retort, and confined reaction tank, and retort is packed into normal pressure gas heating furnace, controls 1000 ± 10 ℃ of furnace temperature; When temperature of charge reaches 800 ℃ ~ 900 ℃, carry out the continuous heating stage, the mode in continuous heating stage is: retort is taken out from gas furnace and pack pressure electrothermal oven into and sealing is fixing, continuous heating to 950 ℃ ~ 1000 ℃;
2) the initial temperature rise period, when material reaches 650 ℃ ~ 700 ℃, passes into nitrogen;
3) temperature-fall period of highest temperature step of reaction after finishing is divided into two stages, the rate of temperature fall of temperature during higher than 650 ℃ is 1 ~ 3 ℃/min, and nitrogen pressure remains on 0.4MPa ~ 1.0MPa, temperature be down to 650 ℃ following after, rate of temperature fall is 3 ℃/min ~ 10 ℃/min, and closes nitrogen valve.
3. the production method of nitrogenized manganese product according to claim 2, is characterized in that, comprises the steps:
1) manganese metal raw material is packed in retort, and confined reaction tank, retort is evacuated to absolute pressure is 50Pa ~ 100Pa simultaneously;
2) mode by the initial temperature rise period makes the temperature of charge in retort rise to 650 ℃ ~ 700 ℃, passes into nitrogen, and to keep retort internal pressure scope be 0.01MPa ~ 0.03MPa;
3) when the temperature of charge in retort reaches 800 ℃ ~ 900 ℃, adopt the mode continuous heating to 950 ℃ in continuous heating stage ~ 1000 ℃, allow the pressure of pressure electrothermal oven internal pressure and retort identical simultaneously, and be controlled at 0.4MPa ~ 1.0MPa;
4) in retort, temperature of charge reaches 950 ℃ ~ 1000 ℃, when nitrogen pressure is 0.4MPa ~ 1.0MPa, and the nitrogen flow that passes into retort be less than peak flow 1% time, control temperature according to the rate of temperature fall cooling of 1 ~ 3 ℃/min, nitrogen pressure still remains on the scope of 0.4MPa ~ 1.0MPa;
5) when the temperature of the material in retort drops to 650 ℃, close nitrogen valve, the pressure of relief pressure electrothermal oven is to normal pressure, and retort is hung out, and packing cooling shaft into, to carry out water smoke air-cooled, controls rate of temperature fall between 3 ℃/min ~ 10 ℃/min;
6), when the temperature of the material in retort is reduced to below 200 ℃, retort is opened in pressure release;
7) pour out material and obtain nitrogenized manganese product, finishing warehouse-in.
4. the production method of nitrogenized manganese product according to claim 3, is characterized in that, manganese metal raw material is any one or the multiple mixing in electrolytic metal Mn sheet, manganese powder, manganese metal ball or metal manganese block described in step 1).
5. the production method of nitrogenized manganese product according to claim 4, is characterized in that, described manganese metal ball is to form by adding water glass pressure forming after the fragmentation of manganese metal sheet.
6. according to the prepared nitrogenized manganese product of any method of right 1-5.
7. nitrogenized manganese product according to claim 6, is characterized in that: the mass content scope of nitrogen is 8% ~ 12%, and the fluctuation of the single batch of product nitrogen content be less than ± 0.5%.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107010610A (en) * | 2017-06-13 | 2017-08-04 | 王兆兵 | A kind of energy-efficient high purity silicon nitride manganese production system |
| CN107140610A (en) * | 2017-06-13 | 2017-09-08 | 王兆兵 | A kind of energy-efficient high purity silicon nitride manganese production method |
| CN107140611A (en) * | 2017-06-13 | 2017-09-08 | 王兆兵 | A kind of new high purity silicon nitride manganese process units |
| CN109536815A (en) * | 2018-11-24 | 2019-03-29 | 冯良荣 | A method of preparing nitridation manganese alloy |
| CN110387479A (en) * | 2019-08-30 | 2019-10-29 | 攀钢集团攀枝花钢铁研究院有限公司 | A kind of preparation method of richness nitrogen manganese titanium base material |
| CN115125392A (en) * | 2022-08-18 | 2022-09-30 | 湘西自治州丰达合金科技有限公司 | Manganese nitride ball production process |
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| CN115125392A (en) * | 2022-08-18 | 2022-09-30 | 湘西自治州丰达合金科技有限公司 | Manganese nitride ball production process |
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